참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Stannous Chloride | HCID 24479 | — |
| 반응물 | 5-Amino-2-chloro-4-fluorophenol | HCID 158654 | — |
| 반응물 | Sodium Nitrite | HCID 23668193 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Sulfuric Acid | HCID 1118 | — |
| 생성물 | 2-Fluoro-4-chloro-5-hydroxyphenylhydrazine hydrochloride | HCID 69142106 | 352.2% |
반응 단계
First, 32.3 g of 5-amino-2-chloro-4-fluorophenol was mixed with 150 ml of concentrated hydrochloric acid, and the mixture was stirred at 50° C. for 30 minutes, to which a solution of 15 g of sodium nitrite dissolved in 40 ml of water was added dropwise at 0° C. over 10 minutes. After stirring at 0° C. for 1 hour, the mixture was cooled to −50° C. Then, a solution of 132 g of tin (11) chloride dissolved in 132 g of concentrated sulfuric acid was rapidly added dropwise at −50° C., and the mixture was gradually warmed to room temperature and stirred for 1 hour. The solids formed were collected by filtration and dried at 80° C. under reduced pressure to give 75 g of the crude 2-fluoro-4-chloro-5-hydroxyphenylhydrazine hydrochloride crystals.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06869913B1 |
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| 출처 데이터셋 | uspto-grants-2005_03 |
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| ORD ID | ord-b3d797874be2464c96341c05c5fda4e3 |
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| 출처 메모 | uspto-grants-2005_03 |
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